LT3752B - Flame retardant composition and method of use - Google Patents

Abstract

A flame retardant composition comprises at least one cyclic phosphonate ester and at least one phosphono amide. The ester and the amide are present in a ratio by weight of 0.1 to 2:1. A co-curing agent (e.g. urea, ethylene urea or an amino-triazine) may be included. The composition may also contain a non-rewetting agent and/or a softening or conditioning agent. The composition is used for the flame retardant treatment of a fabric by first impregnating the fabric with an aqueous solution of the composition and then heating the impregnated fabric at at least 100 DEG C and under acid pH conditions.

Description

The present invention relates to compositions which slow down the ignition and to methods which reduce the combustion of textile materials by these compositions.

The combustion of cotton fabrics is slowed down by the incorporation of various chemicals into these fabrics, which make them worse for longer or shorter periods of time.

U.S. Pat. Nos. 2983623, 4068026, 4078101, 4145463 and 4494951 describe treatment of cotton fabric with tetrakis (oxymethyl) phosphonium compounds or precursors of their condensation with urea. In British application no. No. 8713224 These compounds, their condensation products with urea or mixtures of urea and this phosphorus organic compound are proposed for use in the treatment of cellulose fiber blends with polyester fibers. Of the other chemicals for tissue impregnation, mention is made of 3- (dimethylphosphono) propionic acid methyl olamide, in which the fabric is impregnated and then cured by heating in an acid medium, usually with an accompanying reagent such as melamine-formaldehyde condensate, to produce a cotton cloth. slower and slightly more resistant to washing. However, cotton-polyester fabrics, especially made up of two or more materials, are much more difficult to burn even than cotton fabrics, even with slight deceleration.

We have developed flame-retardant compositions and methods of using them in cellulose and other fabrics, which allow for more flame-resistant and stronger fabrics.

The present invention provides a composition for reducing combustion comprising:

(a) at least one cyclic ester of phosphonic acid I represented by formula (A):

'«V?

^εμ 2.- ° \?

och ₂ C (. ^x ₂ ch o / - R '(A) wherein a is 0,1 or 2, b is 0,1 or 2, c is 1,2 or 3 and a + b + c is 3;

R and R ¹ may be the same or different and are alkyl, alkoxy, aryl; aryloxy, alkylaryl, alkylaryloxy, arylalkyl, aryloxyalkoxy or arylalkyloxy, wherein the alkyl portion of these groups may have at least one hydroxyl but not halogen and the aryl portion may have one chlorine or bromine atom or one hydroxyl group; R ² is alkyl, hydroxyalkyl or aryl; and R ³ is lower alkyl (e.g. C _x -C ₄ ) or hydroxyalkyl (e.g. C ₁ -C ₄ ) or a cyclic phosphonic acid ester represented by formula (B):

R 0, CW 10,

COCH2C

PR '(B)' CH, wherein d is 0,1 or 2; e is 1,2 or 3; d + e equals 3; R is as described above; R also, coincides with the meaning given above; R ⁴ may be alkyl, aryl, alkylaryl, arylalkyl or aryloxyalkyl, the aryl portion of which may or may not contain at least one bromine or chlorine atom or hydroxyl; and R ⁵ is a trivalent hydrocarbyl (hydrocarbon) radical in which, when aromatic but not necessarily one chlorine or bromine atom, one alkyl or hydroxyl group; and (b) at least one phosphonic acid amide represented by the formula

R ⁸ O 7 I

R op-CH -CH ₂ -CO-NH-CH ₂ or wherein R ⁶ is a hydrogen atom or an organic radical and R and R, which may be identical or different, is an organic radical and R ⁹ represents a hydrogen atom or halogen, or an alkyl group or a group represented by the formula CH ₂ CONHCH ₂ OR ⁶ .

The present invention also provides a method for slowing down the combustion of cloth by combining impregnation of a fabric made of cellulose or other fibers with an aqueous medium of a flame retardant composition of the present invention followed by heat treatment of the impregnated cloth at a temperature of at least 100 ° C.

The cyclic ester of phosphonic acid I is described in U.S. Pat. 3849368 and no. No. 3789091, the disclosure of which is hereby incorporated by reference. This ester can be obtained as described in these patents by reaction of complex esters of phosphoric acids, carbonyl acids or sulfanyl acids, in addition to an alkyl halogen, with a bicyclic phosphite such as 1-alkyl-4-phospho-3,5,8-trioxabicyclo- [2 , 2,2] -octane, time. Alkylated, alkoxy or substituted alkylated groups R and R ^ R ⁵ may have from 1 to 6 carbon atoms, while at the same time aryl groups may be aromatic hydrocarbonyl groups having from 6 to 19 carbon atoms and arylalkyl groups may be carbonyl (hydrocarbon). groups and have 7 to 19 carbon atoms. R and R ¹ examples are C ₁ _ ₁₈ alkyl, phenyl, halophenyl, hydroxyphenyl, tolyl, xylyl, benzyl, phenethyl, hydroxyethyl, and _

dibromophenoxy-methyl. R examples are C _x _ ₄ alkyl, phenyl, halophenyl, hidrooksifenilas, hydroxyethyl, phenoxyethyl, dibromfenoksietilas, tolyl, xylene, benzyl or phenethyl, where at the same time R ⁵ examples are C ₁ _ ₆ -alkanarba alkentrinilinės groups and tri radicals derived from benzene optionally substituted with one, two or three bromine or chlorine atoms, one or two C _{x 4} alkyl groups, for example methyl groups or hydroxy groups, or naphthalene. Preferred among all compounds of formula 1 are compounds wherein each of R ¹ and R ¹ , which may be the same or different, is lower alkylated or lower alkoxy, for example from 1 to 6 carbon atoms, especially from 1 to 3 carbon atoms, especially methyl , ethyl, methoxy, ethoxy, where at the same time each R and R, which may be the same or different, is preferably an alkyl group, for example from 1 to 6 carbon atoms such as a methyl group or an ethyl group. Mixtures of cyclic phosphonates may be used in the composition. In the mixture of two phosphonates, the phosphonates are used in a ratio of 95: 5 to 5:35, for example 25:75 to 75:25, especially the first phosphonate wherein a, b and 1 are, and the second phosphonate, where a is equal to 1, b is is equal to 0 and c is equal to 2, in addition, each of the groups R, R ² , R ³ independently on one phosphonate is the same as the corresponding groups on the other phosphonate.

The best mixtures are obtained by mixing in a ratio of 40:60 to 60:40 two phosphonates in which each R,

R ² and R ³ are methyl or ethyl and R ¹ is methoxy or ethoxy such as is described in U.S. Pat.

No. 3849368 of Example 1b, in particular wherein R and R ³ are 2 liters methyl, R is ethyl and R is methoxy. An example of such a mixture would be a mixture obtained by mixing 50:50 parts by weight of phosphonates (wherein R 1, R ³ is methyl, R ¹ is methoxy and R ² is ethyl) sold by Albright & Wilson Americas Ine. under the name ANTIBLAZE 19 or by Albright & Wilson Limitted under the name AMGARD CU.

Phosphonic acid amides are known (see, for example, British Patent Nos. 1011572 and 1139380) and the disclosure herein discloses their essence. In the phosphonic acid amide (phosphonamide) hydrogen is preferably used as the R ⁶ group, but an organic radical is also suitable, for example from 1 to 10 carbon atoms such as an alkyl or alkenyl group, in particular an alkyl group of 1 to 4 carbon atoms , such as methyl, ethyl, propyl or butyl or allyl. R and R, which are preferably the same, form an organic group, for example, from 1 to 13 carbon atoms such as an optionally substituted alkyl group or an alkenyl group, for example, each of 1 to 6 carbon atoms, an aryl group, for example, 6-13 carbon atoms, the cycloaliphatic group being, for example, 5-7 carbon atoms. Examples of such most suitable groups are the methyl or ethyl groups which are the best, the propyl and butyl groups and the derivatives of the monochloro or mono-bromo or chlorobromo alkyl groups which are particularly suitable, and especially the halogenated derivatives thereof. alkenyl groups containing 4 carbon atoms; and ha9 logenylated phenyl groups. R can be hydrogen or halogen, for example a chlorine atom or an alkyd group, for example from 1 to 6 carbon atoms such as methyl or ethyl, or a group of the formula CH ₂ CONHCH ₂ OR ⁶ where R ⁶ is as is as defined above, and is preferably when R ⁶ is hydrogen. A suitable phosphonoamide is propionic acid 3 (dimethylphosphono) methylamide of the formula (CH ₃ O) ₂ POCH ₂ CH ₂ CONHCH ₂ OH.

The weight ratio of cyclic phosphonate to phosphonamide in the composition is usually from 0.1 to 2: 1, for example from 0.2 to 1: 1.

Phosphonoamide hardening agent is used in the compositions to slow down the combustion. As heat-inducing agents, formaldehyde containing a polyfunctional nitrogen compound with at least two NH groups such as urea or amino-triazines such as melamine or cyclic compounds such as ethylene urea or acetylenedicarbamide and / or other nitrogenous compounds is preferred. condensates do not necessarily have to be esterified. Preferably, the curing agent is optionally etherified methylol melamine with 3-6 methylol groups (or their ethers) or optionally etherified methylol tetracitylenedicarbamide. The hardening agent is usually present in an amount of 5 to 30% by weight. %, for example 10-25% by weight. % based on the dry weight of the phosphonamide.

The optional esterification or partially alkylated methylolmelamine hardening agent (also called triazine) consists of a 1,3,5-triazine nucleus and three amino groups at position 2,

4, 6, and typically having an average of 3-6, for example

3.5-6, especially 4-5.5 hydroxymethyl groups, and these hydroxymethyl groups may be present in the form of at least alkyl ethers. Typically, the triazine hardens for 15 minutes, for example at 70 ° C for 40 minutes. The cure time was determined as follows.

0.8 g of 50% by weight was added to a 20 g aqueous solution of triazine containing 80% solids. zinc nitrate hexahydrate solution and stirring constantly until a clear liquid is obtained, and then the vessel containing the solution was kept in a room at a constant temperature of 70 ° C for a period of time (hereinafter referred to as cure time) until the solution solidifies. for a metal spatula. Initial pH of the clear solution Usually 5.8-6.2. If necessary, adjust the pH of the aqueous triazine solution or the clear solution by adding nitric acid or sodium hydroxide, raising the final pH of the clear solution to 5.8-6.2.

Hardening time at 70 ° C can usually range from 15 minutes to 10 hours, such as 40 minutes to 10 hours, for example 40 minutes to 6 hours, such as 40 to 200 minutes or 40 to 140 minutes and especially 40 to 75 minutes. minutes or 70-140 minutes. Preferably at least several hydroxymethyl groups are triazine esterified, for example from 10 to 100%, and in particular from 30 to 80% or 30 to 60% by alkyl groups, for example from 1 to 10 carbon atoms such as from 1 to 5 carbon atoms, e.g. metal, ethyl or butyl groups. As the number of hydroxymethyl groups per triazine nucleus increases, the degree of esterification usually increases. That way, on average

For the 4.5-5.5 hydroxymethyl groups, the degree of alkylation may be 30-60%, and for the average 5.5-6 groups this degree may be 60-90%. The triazine molecule may contain an average of 3-6 or 3.5-6, preferably 4-4.5 alkoxymethyl and hydroxymethyl groups; on average 0.1-4, for example 0.5-2 or 1-3.5, and in particular 1.5-3.5 hydroxymethyl group molecules; and an average of 1-5,9, for example 4-5.9 or 1.5-5, most preferably 1.5-3.5 alkoxymethyl group molecules. The number of hydroxymethyl groups per triazine nucleus and the degree of esterification required are usually based on the number of moles of formaldehyde and alcohol used in the production of triazine, but can be determined by physico-chemical methods of analysis. Esterification is effected by reaction of hydroxymethyl-melamine with the corresponding alkanol under the action of an acidic catalyst. The triazine compound is preferably in the form of a monomeric substance, but may also be present in a small amount in the form of condensate of the monomer, and preferably in the form of 55-100%, e.g. 70-90%, monomeric and 45-0%, e.g. . Examples of commercially available but not necessarily partially alkylated methylimelamines include: BT370 sold by British Industrial Plasics with a cure time of 264 minutes at 70 ° C, partially methylated with hexamethylolmelamines ClBAMIN ML 1000 CB, sold by Cibi Hahi with a cure time of 70 ° C is 290 minutes, but most preferably one which is partially methylated with methylimelamines and is sold by British Industrial Plastics as BT 336, BT 338 or BT309 with a cure time of 70 ° C, 50, 25 and 23 minutes respectively, or such as LIOFIKS CH sold by Ciba Hahi and cured at 70 ° C for 108 minutes.

For ready-to-use formulations, the pH at the start of treatment is less than 3, but the preferred pH is

1.4-2.5. Strong inorganic acids, such as sulfur, salts, and preferably phosphorus, may be used to adjust pH, but compounds which form an acid in an aqueous composition, such as salts with an acidic reaction, such as ammonium chloride, or compounds which hydrolyze acid such as chloro anhydrates of inorganic or organic acids.

The flame retardant composition may include a fluorocarbon polymer (capable of heat curing at temperatures above 160 ° C, for example 160-200 ° C). The fluoro carbonic polymer forms a dispersion in the flame retardant composition which is usually stable for several days, at least 2 days. Fluoropolymers which are incompatible with a solution of phosphonoamide and cyclic phosphonate and which precipitate after mixing shall not be used. Suitable water-dispersible polymers usually have perfluoroalkyl side chains, for example perfluoro-acylic, sulfonyl or sulfanamide groups, in particular 3 to 12 carbon atoms in the perfluoroalkyl group; carboxy groups may be present. Fluoranglical polymers are preferably obtained from acrylic or methacrylic complex ester hydroxy compounds with perfluoroalkyl groups, but may be obtained from complex vinyl esters, vinyl esters, complex allyl esters or thiomethacrylates with perfluoroalkyl side chains. Particularly preferred are polymers having a (N-alkyl N-perfluoroalkylsulfonamide) -alkyl side bond to an acrylate or methacrylate complex ester linkage. Polymers can only be obtained from monomers with perfluoroalkyl groups. On the other hand, these monomers are copolymerized with other fluoropolymerizable monomers, for example monomers having one or two olefinic double bonds, such as halo LT 3752 B butadienes such as 2-chloro-1,3-butadiene. The polymer may have olefinic monomeric units with carboxylic acid groups such as acrylic, methacrylic or maleic acid groups. Fluorine-containing polymers are commonly sold in the form of aqueous dispersion, for example in the form of fluoropolymer dressings for use in the manufacture of non-lubricated fabrics.

The polymeric dispersion may be nonionic, but cationic or anionic, which is particularly suitable, are preferred. Fluorine polymer dispersions may also contain small amounts of organic solvents such as acetone methyl isobutyl ketone or ethylene glycol miscible with water. Fluoropolymer dispersions SKOTCHCARD 270 sold by ZM Compani or SKOTCHCARD DC 451 sold by Ciba Hahi may be used. This polymer is believed to be a copolymer of acrylic acid 2- (N-alkyl N-perfluorooctylsulfanylamide) -ethyl ester and probably a comonomer of 2-chloro-1,3-butadiene. Another suitable fluoropolymer dispersion is marketed by NUVA FH or NUVA F by Hoechst AC. Also, fluoropolymer dispersions FORAPERLE sold by Atochem SA, in particular FORAPERLE 145 and 344, may be used; or TEXFIN CPC, sold by Texshem UK Ltd. of Manchester, England. The percentage by weight of the fluoropolymer, if used, is usually from 0.1 to 5%, for example from 0.2 to 2%, based on the amount of phosphamide. However, fluoropolymers are generally not used in the combustion retardant composition of the present invention.

A wetting agent such as a volatile wetting agent such as alcohol or a MIKON NRW reagent sold by Warwick Chemicals may be included in the composition. However, if the substrate u

(material) which has to be treated to slow down the burning rate, has already been washed or otherwise treated to improve fluid penetration, such an element is unnecessary but can be used if desired. Especially when the composition contains a fluoropolymer and the aqueous medium is usually free of fillers or cationic polymers such as cationic synthetic resin waxes such as CEROL sold by Sandoz and usually no di-, tri- or tetra-valent metal such as aluminum or zirconium, salts. Fluoropolymer dispersions containing a filler or a cationic polymer are also commercially available, but are best avoided. Fluoropolymer dispersions are predominantly marketed as an agent used in the manufacture of non-woven, non-waterproof and non-woven fabrics, and may therefore be incompatible with an aqueous flame retardant composition.

If the fluoropolymer is to be included in the composition, it is preferably added thereto when the composition is ready for use prior to wetting the fabric and may be used for several days, although if anionic fluoropolymer dispersions are used, the composition may be stable for at least a week, for example one month.

Other textile excipients may be present in the aqueous composition, but it is important that they are in nature and quantity compatible with the other components of the composition and that they are slightly modified by heating during curing, for example they must not discolour the fabric. Such excipients include impregnation enhancers and water softeners, which may be cationic, anionic, nonionic, amphoteric or reactive and are typically composed of at least 1, and often 2, alkyl chains of at least 10 carbon atoms.

Fatty tetraammonium salts, complex amino esters and aminoamides and tetra N-acyl N-polyoxyalkylene polyamines are used as cationic emollients. Examples of anionic emollients include fatty acid salts, soaps, sulfated fats and oils, fatty alkoxates and fatty acid condensation products sulfasuccinates and sulfasuccinamates. Examples of amphoteric emollients include alkylimidazolines and betaines, and salts thereof such as methasulfate, acylamido-betaines, acyl-polyamines, amine oxides, displacement amino acids, and sulfabetaines. Simple and complex esters of polyalkylene glycols and paraffin waxes or polyethylene waxes can be used as nonionic softeners, and the latter two can be used in aqueous dispersion or emulsion together with nonionic, cationic or anionic and especially amphoteric dispersing agents. Examples of reactive emollients are N-methylol derivatives of fatty amide acids, for example N-methylolamide of stearic acid or condensates of N-methyl fatty acids with urea. Nonionic softeners based on modified product condensation of melamine and formaldehyde are preferred. 0.01 to 5%, for example 0.5 to 3% by weight, may be used in the compositions. % is the amount of softener determined from the total amount of aqueous impregnation medium.

The use of a softener in the composition can improve fabric properties, degrade ignition, increase strength, especially for tearing, after a curing procedure in a hot environment, and the color remains unchanged, as with untreated fabric.

Composition-coated substrates may be woven or nonwoven. Cellulose-based materials, textiles of cotton, wool, linen, jute or reconstituted cellulosic material, such as artificial silk or rayon, and other fibers obtained by mixing or blending fibers such as polyester or nylon, acrylic, polypropylene may be used fibers, silk or wool. These composite blends or blended component materials may contain at least 30%, for example 30-100% or 30-90%, but preferably at least 40%, for example 40-75%, and particularly preferably at least 50% cellulosic material, for example 50-90%, 50-80% or 70-90%.

Fabrics made of non-composite cellulosic material, such as cotton, polyester (complex polyester) or nylon, are the most suitable for processing.

The fibers used to form at least a portion of the fabric may be woven into the base structure, if desired, but preferably not. The fabrics are blended, for example, a woven fabric and a base, preferably (for example, 50-100%), of a synthetic polymer, for example, with a base of a complex polyester; a sophisticated polyester backing and a cotton weft, especially when combined with embroidered cotton designs, are the most suitable. Exposure to such mixed fabrics which are not treated with a cyclic phosphonate may cause the complex polyester to shrink and melt, unlike cotton, and may catch fire, thereby degrading the fire resistance of all fabric used in the upholstery industry. The flame retardant compositions implemented in accordance with the present invention and the method provide a more uniform flame retardant, at least in part, in such patterned fabrics, particularly fabrics having unevenly distributed synthetic and cotton fibers, which will hereinafter be referred to as non-uniform fabrics.

Of particular interest are non-homogeneous fabrics which have a cellulosic material on the right side that is different from the synthetic polymer content (usually less cellulosic material) and, on the contrary, a synthetic polymer has a lower surface area than cellulosic materials and on the sides, large areas where, for example, 50-100% are made of synthetic fiber and, as a rule, there are zones of cellulosic material occupying 100-50% of the fabric. Such fabrics having a non-uniform surface may include fabrics with a base of a complex ester and dyed cotton weft, in particular with more than one differently dyed cotton weft, as well as fabrics with a right-hand side pattern of such dyed cotton on a polyester backing, without drawing with large cotton surface. Such non-uniform fabrics can also be used as upholstery.

The weights of fabrics to be treated can range from 0.050 to 1.0 kg / m, for example 0.080 to 500 kg / m. Each of the fabric components may be plain (non-patterned) or colored, in particular white or pastel. Before soaking, the cloth is removed from dirt, glue, natural waxes, although the brightening agent may be left behind.

The composition comprises 10-300 g / l, preferably 50-100 g / l of cyclic phosphonate, in the conventionally dry state, for slowing down the combustion; 50-600 g / l, preferably 100-250 g / l phosphonoamide; 5-100 g / l, for example 15-60 g / l, is not necessary, but is desirable to cause the composition to solidify; 10-50 g / l of acid added to adjust the pH to 1.5-3; 5-50 g / l of optional softener, especially jet softener, and 1-20 g / l, e.g. 0.1-5 g / l, for improving fabric impregnation reagent.

An aqueous solution of the flame-retardant composition or further diluted with water, if necessary, and the solution of pH less than 3 is applied by spraying, impregnation, in one of the known ways, up to 50-150%, for example 60-110%. % dry weight of substrate. The amount of solids adhering to the fabric prior to drying and after draining excess fluid is typically 10-30%, for example 10-20% or 13-25% of the weight of the initial fabric.

The impregnated material is dried at 60-140 ° C, for example 90-130 ° C, for 20-0.5 minutes, for example 10-0.5 minutes. Drying can be carried out in well-known dryers, such as an artificial air circulation dryer or a stent. Solids bound to the fabric after drying Usually 8-25%, for example 10-20% of the weight of the initial fabric.

The dried substrate is then cured, for example by heating at a temperature of at least 100 ° C, such as 140-170 ° C, for example for 10 to 0.5 minutes, and avoiding the curing of the substrate at high temperatures for extended periods to minimize discoloration. Thus, the preferred temperatures are 150-170 ° C and the optimum curing time is 5-2 minutes. The use of fluoropolymers in the composition can reduce fabric smear.

Curing, which is usually a continuous process, is accomplished by utilizing heat sources such as infrared heater or steam and / or hot air passing through the substrate, or by compressing the solidified material between metal heated drums, but preferably the substrate hardens by heating the material surface with hot air. current and both surfaces of the material to obtain continuous heating. Thus, it is preferable for the substrate in the stent to be continuously passed through a thermostatic furnace in which heated air flows on both the upper and lower surfaces of the substrate. In the stent, the material hardens uniformly and does not burn. With a stent furnace, the substrate temperature is almost equal to the hot air temperature. At the end of curing, the substrate is cooled either by supplying additional or by aspirating cold air. The resulting cloth is washed with alkaline solution and water.

The cured fabric after washing is typically 6-25%, for example 8-20% solids, and usually 0.5-4%, but is preferably 1-3%, 1.5-2.5% or 24% P (phosphorus).

The resulting fabric, as compared to fabric untreated with the compositions described, is difficult to ignite and can be tested by BS 5852 with Class 0 and Class 1 combustion sources. The resulting coating is stable and resistant to washing. The cloth is used and maintained just like the raw cloth.

The synergistic alignment of the cyclic phosphonate (a) and phosphonoamide (b) allowed the fabrics to exhibit increased flame resistance and strength, which are not obtained in fabrics treated solely with material (a) or (b).

The following examples illustrate the present invention.

Example No. 1

The aqueous impregnation fluid is prepared by mixing, in the order indicated, the following ingredients, also listed below: 225 g / l 80% solution of 3- (dimethylphosphonic) propionic acid methylolamide, 40 g / l 80% partially esterified melamine-formaldehyde condensate BT338 sold by British Industrial Plastics, 25 g / l 88% phosphoric acid, 15 g / l nonionic softener, based on modified melamine formaldehyde condensate TURPEKS NPF sold by Cibe Hihi, 1 g / l impregnation enhancer Mikon NRW sold by Warwick Chemicals , and 70 g / l of cyclic phosphonates AMGRARD CU or ANTIBLAZ 19 (see description above). Mixed fabric consisting of 65% cotton and 35% polyester, 0.335 kg / m, was impregnated with a polyester backing in a calender aqueous solution to obtain a fabric saturated composition gradient and a wet weight of 95% The dry weight of the impregnated cloth is dried in a stent with an artificial air circulation at 100 ° C for 2 minutes. The dried cloth is pulled through a stent, through a Benco dryer, in which hot air flows from the top and bottom of the fabric. The curing time was 3 minutes at 160 ° C.

The moistened cloth was washed in a tub in successive 20 g / l, 10 g / l sodium carbonate solutions followed by hot and cold water. The cloth was then dried and tested for flammability using the 0 and 1 ignition sources according to Part B of Test B5952 (1979) and tested in Part B of Test B5651 after basification in hard water at 40 ° C.

Comparative example

In the comparative example, the method described in the first example identical to the first device from which the phosphonate was cyclically removed was repeated. The cloth did not pass the flame resistance tests before and after the alkalization.

Examples 2 and 3

Samples of a mixed fabric consisting of 55% cotton and 45% polyester and 0, 330 kg / m were further processed using the method described in the first example to retard the ignition of the cotton-polyester upholstery fabric.

The treatment was carried out with the composition as in the first example except for the AMGARD CU attachment:

225 g / l 3- (dimethylphosphono) -propionic acid methyl olamide (80%);

g / 1 B T338;

g / 1 TURPEKS NPF;

g / l phosphoric acid (88%);

g / 1 MIKON NRW (Composition A).

The following formulation was used as a base for 3 assays using Composition A with 50 g / l AMGARD CU - Composition B and 100 g / l AMGARD CU - Composition C. The impregnation, drying, solidification and washing processes were performed. as described in Example no. 1 before drying and testing.

Test results

The samples were treated with formulations A and B and then tested in BS 5852 Part One (1979) using Type 0 and Type 1 ignition sources to determine fabric resistance to fire and to run before and after washing in hard alkaline water as described in BS test. 5651, before cloth leveling.

The sample treated with composition A did not pass the above flammability tests.

Claims (24)

DEFINITION OF INVENTION An inflammatory composition comprising combining: (i) at least one cyclic phosphonate complex ester of formula (A) ČHzOCHI A p R · '(L) (R) a CHf 0 'wherein a is 0,1 or 2, b is 0,1 or 2, c is 1,2 or 3 and a + b + c is 3, R and R ¹ may be the same or different and are alkyl, alkoxy -, aryl, aryloxy, alkylaryl, alkylaryloxy, arylalkyl, aryloxy, alkoxy or arylalkyloxy, the alkyl moiety of which may have at least one hydroxyl but not halogen and the aryl moiety may have one chlorine or bromine atom, or one hydroxy hydroxy group, R is alkyl, hydroxyalkyl or aryl, and R ³ is lower alkyl (e.g. C ₁ -C ₄ or hydroxyalkyl (e.g. Ο _χ- Ο ₄ )), or a cyclic complex phosphonic acid ester of formula (B) - 0 5 * this R - 7oc (B) wherein d is 0,1 or 2, e is 1,2 or 3, d + e is equal to 3, 2 3 R is as defined above, R is also as defined above, R ⁴ may be alkyl, aryl, alkylaryl, arylalkyl or aryloxyalkyl, the aryl moiety of which may or may not contain at least one bromine or chlorine atom or hydroxyl, and R ⁵ is a trivalent hydrocarbyl (hydrocarbon) radical in which, when aromatic but not necessarily one chlorine or bromine atom, one alkyl or hydroxyl group, and (ii) at least one phosphonamide of the formula R ⁸ O i I R op-ch ₂ -ch-co-nh-ch ₂ or wherein R ^{6 *} is a hydrogen atom or an organic radi-y g cal, and R and R, which may be the same or different, are an organic radical and R is a hydrogen atom or a halogen or an alkyl group or a group of the formula CH ₂ CONHCH ₂ OR ⁶ . 2. A composition according to claim 1, characterized in that the characterized in that R and R ¹ independently is C _x _ ₆ alkyl or alkoxy -group, such as methyl, methoxy, ethyl or ethoxy. 3. The composition according to claim 1 or 2, which opens besiski2 3 in which R and R are independently C _x _ ₆ alkyl such as methyl or ethyl. Composition according to claims 1-3, characterized in that component (i) consists of a mixture of cyclic phosphonates, for example one phosphonate of formula (A) and wherein a = 1, b = 1 and c = 1 and the other a phosphonate of formula (A) and wherein a = 1, b = 0, and c = 2 and each • 1 3 2 R, R and R, R are the same in each phosphonate. 5. A composition according to claim 4, wherein the weight ratios of the components of formula (A) are from 40:60 to 60:40, and R, R ² and R ³ are methyl or ethyl and R ¹ is methoxy or ethoxy. . 6. The composition of claim 5, wherein the weight ratio is 50:50 and R and R ³ are methyl, R ¹ is methoxy and R ² is ethyl. 7. A composition according to claims 1-6, characterized in that the characterized in that R ⁶ is hydrogen or a C? -C? Alkyl, or alkenyl, for example, C ₁ _ alkyl, or _J alililas. 8. A composition according to claims 1-7 characterized in that the characterized in that R and R are each independently optionally substituted by C _x _ ₁₃ hydrocarbon group such Cj.4 alkyl, C ₂ _ ₄ alkenyl, or phenyl optionally substituted with one or more halogen atoms. 9. A composition according to claims 1-8, wherein R is hydrogen, halogen, C _1-4 alkyl or CH ₂ CONHCH ₂ OR ⁶ such as methyl or ethyl. 10. The composition of claims 1-9, wherein component (ii) is (CH ₃ O) ₂ POCH ₂ CH ₂ CONHCH ₂ OH. 11. The composition of claim 1, wherein the weight ratio of component (i) to component (ii) is from 0.1: 1 to 2: 1, for example from 0.2: 1 to 1: 1. 12. The composition of claim 1, wherein a hardening agent for component (ii), such as urea, aminotriazine, ethylene urea, acitylenedicarbamide, optionally esterified formaldehyde condensate thereof, or a mixture thereof, is added. 13. The composition of claim 12, wherein the curing agent has a cure time greater than 15 minutes. 14. The composition of claim 1 further comprising a fluoropolymer. 15. The composition of claim 14, wherein the fluoropolymer is composed of a sulfonamide group N-alkyl-N-perfluoroalkyl, for example C ₃ H ₇ C ₈ F ₁₇ SO ₂ NH-. 16. A composition according to claim 1, further comprising an impregnation enhancer and / or a cationic, anionic, nonionic amphoteric or reactive emollient or conditioning agent. 17. The composition of claim 1, wherein the pH is less than 3. 18. A method of retarding the ignition of a fabric by incorporating in said fabric a chemical that impairs its combustion, characterized in that the fabric consisting of cellulosic and non-cellulosic fibers is impregnated in an aqueous, anti-inflammatory composition, solution and heat treated in accordance with claims 1-17. , at a temperature of at least 100 ° C. 19. The method of claim 18, wherein the fabric comprises 50-90% (e.g., 70-90%) cellulosic material. 20. The method of claims 18-19, wherein the fabric is a mixed fabric (for example, a woven fabric consisting of cotton and a base of polyester or nylon). 21. The method of claims 16-20, wherein the fabric has a non-uniform surface. 22. The method of claims 18-20, wherein the fabric is soaked until its moisture content is increased by 50 to 150% or 10-35% by weight of solids. 23. The method of claims 19-22, wherein the fabric is heat treated for 5 to 2 minutes at 150-170 ° C. 24. The method of claims 18-23, wherein the amount of phosphorus in the fabric after treatment is 0.5-4% by weight.